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Two new chiral stationary phases, 2,3-di-O-acetyl-6-O-trimethylsilyl-β-cyclodextrin (DATBCD)and 2, 6-di-O-trimethylsilyl-3-O-acetyl-β-cyclodextrin (DTABCD), were synthesized, their structures were identified by memos of infrared and NMB spectra. Capillary columns were coated with the two stationary- phases by dynamic method. The chromatographic properties, and enantiomers separation, such as ketone, esters, alcohols and olefines, were investigated on the silylated and acetylated β-cyclodextrin stationary phases. The expehmental results show that the silylated and acetylated β-cyclodextrins are suitable to be used as capillary gas chromatographic stationary phases, the relative polarity of DATBCD and DTABCD stationary phases is respectively 4143 and 3928, the colmnn efficiencies are respectively 3084 and 4198, and DATBCD is of stronger enantioselectivity- than DTABCD, capacity factor of the first eluted enantiomer ( k1 ) and separation factor(α)of α-phenylethanol on DATBCD stationary phase are respectively 8.23 and 1.019.